Process for the production of catalytic material and the saturation of fatty acids or their glycerids with hydrogen.



Israe HARIIEY J. MORRISON, OF CINCINNATI, OHIO, ASSIGNOR, BYMESNE-ASSIGNMENTS, TO

THE HYDROGEN ATION COMPANY, OF CINCINNATI, OHIO, A CORPORATION OF OHIO.

rnocnss r012. THE PRODUCTION or cATA'LYTIc MATERIAL AND THE SATURATIONor FATTY ACIDS on THEIR GLYOERIDS wITn HYDROGEN.

No Drawing.

T 0 all whom it may concern:

Be it known that I, HARLEY J. MORRISON, a citizen of the United States,and a resident of the city of Cincinnati,in the county of Hamilton andState of Ohio, have invented a certain novel and useful Process for theProduction of Catalytic Material and the Saturation of Fatty Acids orTheir Glycerids with Hydrogen, of which the following is aspecification.

It is well known that unsaturated fatty acids, glycerids and otheresters .may be hydrogenized or converted into corresponding Saturatedcompounds by treatment with hy drogen in the presence of catalyticmaterial. In this treatment, it. has been most usual to employ as thecatalyzer such finely-divided metals as have been found to pomess therequired catalytic efficienpy, and among other metals,finely-dividednlckel has been found the most practical and commercially availablemetal for this purpose, although. in my present invention, I do not wishto confine myself to nickel catalytic material alone. As the efiiciencyof-the ,catalyzer apparentlydepends to a large extent on itsfinely-divided condition, much difficulty has beeen met with in thepreparation of. an efi'ective and reliable catalyzer adapted forcommercial use, and in the preparation, for

. example, of powdered nickel from nickel salts, much time, labor andcare are required.

The usual method for the saturation of fatty acids, their glycerids andother esters is to introduce into a suitable vessel the material to betreated with a small percentage of catalyzer, and then to treat the masswith hydrogen, to convert the material into the desired saturated orpartially saturated 0on dition.

I have, however, discovered that, the production of the catalyticmaterialfrom substantially non-catalytic salts or reducible compounds ofthe base catalytic metals, and the saturation process may be carried onin one operation, and that underproper -conditions and treatment in themanner to Specification of Letters Patent.

Patented Apr. 1, 1919.

Application filed September 11, 1912. Serial No. 719,761.

hereinafter fully set forth and claimed, the catalyzer may be formed ata much lower temperature than heretofore required and in 150 much lesstime, and the fatty acids may be saturated or partially saturated in onecontinuous operation with the preparation of the catalyzer. 1

I have discovered that carbonates, oxids 56 and hydroxids of the metalsfrom which catalyzers have been heretofore derived, and whichcarbonates, oxids and hydroxids in then'iselves have little or nocatalyticv effect, may be employed, mingled with the unsat- 60 uratedmaterial in the same manner as catalytic material has been heretoforeused, and when treated withhydrogen under the proper conditions oftemperature and pressure, the metalliferous material will be reduced andrendered catalytic, and the saturating of the unsaturated material willproceed immediately and continue to any desired point. It is notnecessary to use absolutely pure or dry materials. Further any of thesoluble salts may be precipitated within the vessel containing thematerial to be saturated as a carbonate or hydroxid. It is preferable,however, to avoid-such salts, the acid portion of which will form areducible salt with .the precipitant, or which salt would act as apoison.

In carrying out my invention, I introduce the oil into a suitable tankor vessel which may be heated by steam coils, oil bath, or I ..drogengas is introduced, the condition of pressurebeing nonessentiaL- Y Withthe introduc of the hydrogen,

the mass is heatedfron .two hundred and fifty (250) degrees C. to twohundred and ninety (290) degrees C. until the desired degree ofsaturation is obtained. Before T introducing the hydrogen, carbonic acidgas. '5 or other inert gas may be introduced into the Vessel to driveout any air or other gases and the mass is properly agitated duringthetreatment with the hydrogen.

The non-catalytic metallic material is prefand the hydrogen on thematerial suspended in the oilin fine1y-divided condition is to re-' duceit gradually to a metallic state, and asit 'is reduced the metal acts asa catalyst commencing the hydrogenization of the fatty acid, glycerid orester immediately.

As an example of the results obtained by this treatment, I take twohundred grams of cottonseed oil in a suitable vessel adapted to beheatedand furnished-with pipes for the introduction and passage of thehydrogen gas and add thereto one grain of dried nickel carbonate. Thematerial is then to two hundred and seventy de ees C.

then pass a current of hydrogen t rough the mass and the treatment iscontinued for two hours. At the end of this time a product is obtainedhaving a melting point of fortyone (41) degrees C., and an iodin valueof 51.0. The reaction was still brisk and a.

much lower iodin value would have been obtamed by longer treatment.

I Second example. L

The same treatment of cottonseed oilwith hoursproduced a fat withmelting point of I thirty,-eight"'(3 8)' degreesiC. and an iodin \valueofj'66. i

Similar results were obtained by thor- "oughly mixing with theoil, wetfreshly-precipitated'car'bonates or hydroxide; also the b ic carbonateprecipitated from a solution of nickel chlorid by sodium carbonate.

Under'my process the nickel carbonate or hydroxid is reduced to ametallic state and it' gis highly magnetic. 1 c Q'By filtering out themetal, an effective era'bly, but not necessarily thoroughly dried beforeit is used, and the efl'ectof the heat agitated and heated to twohundred and fifty three per cent. of copper hydroxid for two catalyzeris ebtained, suitable for subsequent operations at the ordinary loyvtem- ,peratures usually employed for saturation.

, As anew method of producing a catalyzer my discovery is of greatimportance.

For thereduction of a nickel salt to the finely-divided metallic statefor a catalyzer under the ordinary processes, the temperature isusuallysix hundred to seven hundred degrees C., and the time required coversmany hours. I

In my present process, the 'oil appears to act as a mechanical separatoror' supporter, holding the metal as formed in suspension and infinely-divided form.

Wherethe production ofa catalyzer alone Y is-desired, a saturated or'nert oil,'such as a 'paraflin hydrocarbon, ma be usedas the support,which oil will not under circumstances abs'orbfhydrogen. Undertheseconditions, the mineral 011 acts as the sup-.

port and the catalytic metal is produced, but there is no absorption ofthe gas during the chemical reaction.

I claim:

1. The method of preparing a metal catalyzer and hydrogenizing fattyacids and their esters in one operation, which consists in agitating aheated mixture of the material to be hydrogenized-and a: substantiallynoncatalytic compound of a catalytlc metal, the.-

process being conducted in an atmosphere containing hydrogen and at atemperature substantially from two hundred-and fifty degrees centigradeto two hundred and ninety degrees centigrade, said compound reducibleunder the conditions of the propess;

2. The method of preparing a metal catalyzer which consists in agitatinga heated mixtiiie of oil an a substantially non-catalytic compound of acatalytic metal in contact with a gaseous reducing agent, the processbeing conducted at atemperature sub stantially from two hundred and,fifty degrees centigrade to/two hundred and ninet degrees centigrade,said compopnd reducible under the conditions of the process.

3.- The method of preparing a catalyzer and hydrogenizing fatty acidsand their esters in one operation, which consists in treating the heatedmaterial'to be hydrogenized with hydrogen in'the presence of asubstantially non-catalytic compound of a catalytic' metal,-the processbeing conducted at a temperature substantially from 'two hundred andfifty degrees to two hundred and ninety degrees centigrade, saidcompound reducible under the conditions of the process.

4. The method of preparing a catalyzer,

which consists in subjecting a heated mix-' ture of'oil and asubstantially non-catalytic compound of a catalytic metal to the actionof a gaseous reducing agent at temperature v v substantially from twohundred and fifty dea gaseous reducing agent at a temperature greescentigrade to two hundred and ninety substantially from two hundred andfifty 10 egrees centigrade, said compound reduc1- degrees centigrade totwo hundred and:

ble under the conditions of the process. ninety degrees centigrade.

5 5. The method of preparing a catalyzer, HARLEY J. MORRISON.

which consists in subjecting a heated m'ix- Attest: f v ture of oil andasubstantially non-catalytic THOMAS BENTHAM,

reducible nickel compound to the action of ANNA F. DIENST.

